HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 60142041, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 4-Chlorobenzenesulfonyl chloride | HCID 7398 | — |
| Reactant | HCID 68295643 | HCID 68295643 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60142041 | HCID 60142041 | — |
Reaction Steps
To 100 mg (0.31 mmol) 2-Methoxy-5-(4-methyl-6-morpholin-4-yl-pyrimidin-5-ylethynyl)-pyridin-3-ylamine (E-9) in 5 mL DCM is added 130 mg (0.61 mmol) 4-chlorobenzenesulfonyl chloride and 72 μL (0.97 mmol) pyridine and the reaction mixture is stirred over night at RT. Water (2 mL) is added, the mixture is shaken for five minutes, the aqueous phase is separated and is extracted three times with 4 mL DCM. The combined organic phases are dried over MgSO4 and concentrated under reduced pressure. The crude product is purified by RP chromatography (C18, 20-80% ACN in water containing 1% formic acid). Yield: 105 mg (76%). HPLC-MS: M+H=500; tR=0.91 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598157B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-425d759a9dca47ba9148e52d00f1b5d8 |
| Source note | uspto-grants-2013_12 |